CN106811227A - 一种利用能源草沼渣制备生物油的方法 - Google Patents
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Abstract
本发明提供了一种利用能源草沼渣制备生物油的方法,该制备方法包括如下步骤:能源草厌氧沼气发酵处理、沼渣洗涤、沼渣烘干、沼渣粉碎、热裂解、热裂解蒸汽冷凝、加氢脱氧反应和加氢裂解反应等步骤。本发明利用沼气工程中排放的废弃物能源草沼渣生产商品化价值很高的生物油,是能源草沼渣在生物能源领域的进一步应用,可以使沼气工程的经济效益提高15%以上。
Description
技术领域
本发明属于生物质综合利用领域,具体涉及一种利用能源草沼渣制备生物油的方法。
背景技术
能源草包括一年生或多年生,高木质纤维素含量,高产量,高光合效率的草本能源植物,是开发潜力巨大的能源植物,已成为沼气工程的主要原料之一。能源草沼渣木质纤维素含量高,而且质地疏松,易于粉碎,适宜在生物能源领域进一步利用。能源草沼渣进一步高值化开发利用是提高沼气工程经济效益的重要途径。但是能源草沼渣一般做有机肥料直接排放到农田,经济效益不高。能源草沼渣可被生物降解利用的有效成分很低,不能通过生物发酵的方法经济高效地转化为生物能源,因此它在生物能源领域的进一步开发利用鲜有文献报道。
生物质热解是目前较有前景的生物质利用处置技术,可将低能量密度的生物质转化为高能量密度的气、液、固产品,其中热解得液态产物通常称为生物油。生物油一般有木料、锯末、农作物秸秆制备而成,因其原料结构致密,预处理过程复杂,且原料成分较为复杂,制备的生物油杂质较多,限制了其应用价值。
发明内容
本发明根据能源草沼渣性质开发出了一套完整高效的生物油生产技术,该方法包括以下具体步骤:
(1)把新鲜能源草、干燥能源草或青贮能源草粉碎到10厘米以下,进行厌氧沼气发酵,原料在发酵罐内滞留时间为中温35-40℃发酵18-45天或高温52℃-57℃发酵8~22天;
(2)发酵结束后,将发酵后的能源草沼渣排出,沥干沼液,沼渣浸泡在重量5~12倍的清水中洗涤3~5次,每次洗涤过程中搅拌3~8次,使能源草沼渣充分浸润,排出的沼液和洗涤液用于沼气发酵或能源草种植;
(3) 将洗涤后的能源草沼渣放入温度45~65℃、体积分数0.8~1.4%的乙酸溶液中,用20~90KHz超声处理20~50 分钟,然后取出沼渣,沥干乙酸溶液,再用清水洗涤3~5次。
(4)将步骤(3)清洗过的能源草沼渣沥干水分,自然晾晒至水分含量5~26wt%,然后在80℃~180℃烘干至含水率0.5~6wt%;
(5)用3000~6000转/分钟的高速切割粉碎机将干燥后的能源草沼渣粉碎至0.7厘米以下的细粉;
(6) 将所得的能源草沼渣细粉进行无氧热裂解,得到热裂解蒸汽,热裂解的方法为快速热裂解、闪速热裂解、真空热裂解和加氢热裂解中的一种;
(7)将所得的热裂解蒸汽通入冷凝器,在依次在20~50℃、10~20℃、-5~10℃、-20~-5℃四个冷凝梯度下冷却形成4种液体。
(8)对凝结的4种液体分别进行800~5000转/分钟离心,分离油相和水相;
(9)对4种油相分别采用Co-Mo或Ni-Mo做催化剂,在反应温度300~500 ℃、压力10~20M Pa条件下,进行加氢脱氧反应和加氢裂解反应,进一步脱除残余的氧原子并降解大分子,得到直接用做燃料或与石化汽油、柴油混合使用的成品生物油。
所述能源草为杂交狼尾草、细茎杂交狼尾草、紫象草、矮象草、红象草、象草、牧草蔗、巨菌草、皇竹草、中国台湾甜草、拟高粱、甜高粱、芦竹、芦苇、类芦、斑茅、彼特草、苏丹草、美洲狼尾草、王草、五节芒、芒萁、香茅、互花米草, 大米草中的一种或几种。
步骤(6)所述快速热裂解工艺参数:升温速度12~20℃/s,反应温度590~760℃,原料滞留时间0.2~6s;闪速热裂解工艺参数:升温速度850~1500℃/s,反应温度500~680℃,原料滞留时间0.2~6s;真空热裂解工艺参数:升温速度1~10℃/s,反应温度250~420℃,原料滞留时间1~35s;加氢热裂解工艺参数:升温速度10~25℃/s,反应温度300~480℃,原料滞留时间0.5~8s。
相对于目前已有生产技术,本发明的优势在于:
(1)本发明根据沼气发酵的能源草沼渣灰分很低的特点,省去了常规原料中利用大量酸液脱灰分的步骤,大大节约了化学试剂的投入,节约了成本。
(2)能源草沼渣质地疏松,容易粉碎,本发明降低了粉碎机的耗电量,而且不需要汽爆等预处理步骤,节约了原料预处理过程中的能源投入。
(3)能源草沼渣木质纤维素含量高,纤维素、半纤维素、木质素比例合适,生产的生物油的不仅出油率高,而且生物油质量好。
(4)本发明利用沼气工程中排放的废弃物能源草沼渣生产商品化价值很高的生物油,是能源草沼渣在生物能源领域的进一步应用,可以使沼气工程的经济效益提高15%以上。
具体实施方式
以下结合具体实施例对本发明做进一步说明,但本发明不仅仅限于这些实施例。
实施例1
一种利用能源草沼渣制备生物油的方法,包括以下具体步骤:
(1)把新鲜能源草粉碎到10厘米以下,进行厌氧沼气发酵,原料在发酵罐内滞留时间为中温40℃发酵18天;
(2)发酵结束后,将发酵后的能源草沼渣排出,沥干沼液,沼渣浸泡在重量5倍的清水中洗涤3次,每次洗涤过程中搅拌3次,使能源草沼渣充分浸润,排出的沼液和洗涤液用于能源草种植;
(3) 将洗涤后的能源草沼渣放入温度45℃、体积分数0.8%的乙酸溶液中,用25KHz超声处理28 分钟,然后取出沼渣,沥干乙酸溶液,再用清水洗涤5次。
(4)将步骤(3)清洗过的能源草沼渣沥干水分,自然晾晒至水分含量16wt%,然后在180℃烘干至含水率1wt%;
(5)用3000转/分钟的高速切割粉碎机将干燥后的能源草沼渣粉碎至0.7厘米以下的细粉;
(6) 将所得的能源草沼渣细粉进行无氧热裂解,得到热裂解蒸汽,热裂解的方法为快速热裂解;
(7)将所得的热裂解蒸汽通入冷凝器,在依次在40℃、15℃、8℃、-12℃四个冷凝梯度下冷却形成4种液体。
(8)对凝结的4种液体分别进行1000转/分钟离心,分离油相和水相;
(9)对4种油相分别采用Co-Mo做催化剂,在反应温度300 ℃、压力10 M Pa条件下,进行加氢脱氧反应和加氢裂解反应,进一步脱除残余的氧原子并降解大分子,得到直接用做燃料或与石化汽油、柴油混合使用的成品生物油。
所述能源草为杂交狼尾草。
步骤(6)所述快速热裂解工艺参数:升温速度20℃/s,反应温度760℃,原料滞留时间0.2s。
实施例2
一种利用能源草沼渣制备生物油的方法,包括以下具体步骤:
(1)把干燥能源草粉碎到10厘米以下,进行厌氧沼气发酵,原料在发酵罐内滞留时间为高温52℃发酵18天;
(2)发酵结束后,将发酵后的能源草沼渣排出,沥干沼液,沼渣浸泡在重量7倍的清水中洗涤3次,每次洗涤过程中搅拌3次,使能源草沼渣充分浸润,排出的沼液和洗涤液用于沼气发酵;
(3) 将洗涤后的能源草沼渣放入温度65℃、体积分数0.8%的乙酸溶液中,用60KHz超声处理35 分钟,然后取出沼渣,沥干乙酸溶液,再用清水洗涤3次。
(4)将步骤(3)清洗过的能源草沼渣沥干水分,自然晾晒至水分含量12wt%,然后在100℃烘干至含水率3wt%;
(5)用3600转/分钟的高速切割粉碎机将干燥后的能源草沼渣粉碎至0.7厘米以下的细粉;
(6) 将所得的能源草沼渣细粉进行无氧热裂解,得到热裂解蒸汽,热裂解的方法为闪速热裂解;
(7)将所得的热裂解蒸汽通入冷凝器,在依次在25℃、15℃、0℃、-10℃四个冷凝梯度下冷却形成4种液体。
(8)对凝结的4种液体分别进行3000转/分钟离心,分离油相和水相;
(9)对4种油相分别采用Ni-Mo做催化剂,在反应温度500 ℃、压力12 M Pa条件下,进行加氢脱氧反应和加氢裂解反应,进一步脱除残余的氧原子并降解大分子,得到直接用做燃料或与石化汽油、柴油混合使用的成品生物油。
所述能源草为红象草。
步骤(6)所述闪速热裂解工艺参数:升温速度1500℃/s,反应温度680℃,原料滞留时间0.2s。
实施例3
一种利用能源草沼渣制备生物油的方法,包括以下具体步骤:
(1)把青贮能源草粉碎到10厘米以下,进行厌氧沼气发酵,原料在发酵罐内滞留时间为中温37℃发酵25天;
(2)发酵结束后,将发酵后的能源草沼渣排出,沥干沼液,沼渣浸泡在重量12倍的清水中洗涤3次,每次洗涤过程中搅拌3次,使能源草沼渣充分浸润,排出的沼液和洗涤液用于能源草种植;
(3) 将洗涤后的能源草沼渣放入温度55℃、体积分数1.2%的乙酸溶液中,用70KHz超声处理30 分钟,然后取出沼渣,沥干乙酸溶液,再用清水洗涤4次。
(4)将步骤(3)清洗过的能源草沼渣沥干水分,自然晾晒至水分含量26wt%,然后在180℃烘干至含水率6wt%;
(5)用3000~6000转/分钟的高速切割粉碎机将干燥后的能源草沼渣粉碎至0.7厘米以下的细粉;
(6) 将所得的能源草沼渣细粉进行无氧热裂解,得到热裂解蒸汽,热裂解的方法为真空热裂解;
(7)将所得的热裂解蒸汽通入冷凝器,在依次在50℃、20℃、10℃、-5℃四个冷凝梯度下冷却形成4种液体。
(8)对凝结的4种液体分别进行4500转/分钟离心,分离油相和水相;
(9)对4种油相分别采用Ni-Mo做催化剂,在反应温度450 ℃、压力18 M Pa条件下,进行加氢脱氧反应和加氢裂解反应,进一步脱除残余的氧原子并降解大分子,得到直接用做燃料或与石化汽油、柴油混合使用的成品生物油。
所述能源草为拟高粱。
步骤(6)所述真空热裂解工艺参数:升温速度10℃/s,反应温度420℃,原料滞留时间35s。
以上所述仅为本发明的较佳实施例,凡依本发明申请专利范围所做的均等变化与修饰,皆应属本发明的涵盖范围。
Claims (3)
1.一种利用能源草沼渣制备生物油的方法,其特征在于,包括以下具体步骤:
(1)把新鲜能源草、干燥能源草或青贮能源草粉碎到10厘米以下,进行厌氧沼气发酵,原料在发酵罐内滞留时间为中温35-40℃发酵18-45天或高温52℃-57℃发酵8~22天;
(2)发酵结束后,将发酵后的能源草沼渣排出,沥干沼液,沼渣浸泡在重量5~12倍的清水中洗涤3~5次,每次洗涤过程中搅拌3~8次,使能源草沼渣充分浸润,排出的沼液和洗涤液用于沼气发酵或能源草种植;
(3)将洗涤后的能源草沼渣放入温度45~65℃、体积分数0.8~1.4%的乙酸溶液中,用20~90KHz超声处理20~50 分钟,然后取出沼渣,沥干乙酸溶液,再用清水洗涤3~5次;
(4)将步骤(3)清洗过的能源草沼渣沥干水分,自然晾晒至水分含量5~26wt%,然后在80℃~180℃烘干至含水率0.5~6wt%;
(5)用3000~6000转/分钟的高速切割粉碎机将干燥后的能源草沼渣粉碎至0.7厘米以下的细粉;
(6)将所得的能源草沼渣细粉进行无氧热裂解,得到热裂解蒸汽,热裂解的方法为快速热裂解、闪速热裂解、真空热裂解和加氢热裂解中的一种;
(7)将所得的热裂解蒸汽通入冷凝器,在依次在20~50℃、10~20℃、-5~10℃、-20~-5℃四个冷凝梯度下冷却形成4种液体;
(8)对凝结的4种液体分别进行800~5000转/分钟离心,分离油相和水相;
(9)对4种油相分别采用Co-Mo或Ni-Mo做催化剂,在反应温度300~500 ℃、压力10~20M Pa条件下,进行加氢脱氧反应和加氢裂解反应,进一步脱除残余的氧原子并降解大分子,得到直接用做燃料或与石化汽油、柴油混合使用的成品生物油。
2.根据权利要求书1所述的一种利用能源草沼渣制备生物油的方法,其特征在于:
所述能源草为杂交狼尾草、细茎杂交狼尾草、紫象草、矮象草、红象草、象草、牧草蔗、巨菌草、皇竹草、中国台湾甜草、拟高粱、甜高粱、芦竹、芦苇、类芦、斑茅、彼特草、苏丹草、美洲狼尾草、王草、五节芒、芒萁、香茅、互花米草, 大米草中的一种或几种。
3.根据权利要求书1所述的一种利用能源草沼渣制备生物油的方法,其特征在于:
步骤(6)所述快速热裂解工艺参数:升温速度12~20℃/s,反应温度590~760℃,原料滞留时间0.2~6s;闪速热裂解工艺参数:升温速度850~1500℃/s,反应温度500~680℃,原料滞留时间0.2~6s;真空热裂解工艺参数:升温速度1~10℃/s,反应温度250~420℃,原料滞留时间1~35s;加氢热裂解工艺参数:升温速度10~25℃/s,反应温度300~480℃,原料滞留时间0.5~8s。
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